Quality control for rubber closures & secondary material

1. By:
Dr. Kavita Bahmani
Assistant Professor
Department of Pharmaeutical Sciences, GJUS&T,
Hisar , Haryana, India
Tuesday, April 21, 2020

2.  Sterility Test
 Fragmentation Test
a. For aqueous preparation
b. For dry preparation
 Self-seal Ability
 pH of aqueous extract
 Light absorption test
 Reducing substances
 Residue on evaporation
Tuesday, April 21, 2020
FOR RUBBER CLOSURES

3. 
Preparation of solution(A) for various tests
Wash closures in 0.2% w/v of anionic surface
active agents for 5 min, rinse 5 times with distilled
water and add 200 ml water & it is suspended to
autoclave at 119 123 ºC for 20-30 min covering
with aluminum foil. Cool and separate solution
from closure
Tuesday, April 21, 2020

4. 
In this test subject treated closure to sterilization at 64-66 ºc
and a pressure of about 0.7 Kilo Pascal for 24 hrs.
Tuesday, April 21, 2020
Sterility Test
It should not become
tacky or soften

5. 
 Place water corresponding to the nominal volume minus
4ml in each of 12 clean vials
 Close the vials with prepared closures & 16 hr allow it to
stand for 16 hr.
 Using a hypodermic needle with an external diameter of
0.8 mm inject 1 ml of water into vial and remove 1 ml of air
 Carry out this operation 4 times with new needle each time
 Pass the liquid in the vials through a filter with a pore size
of 0.5µm
 No. of fragments NMT 10 except in the case of butyl
rubber closure where the total no. of fragments NMT 15
Tuesday, April 21, 2020
Fragmentation test
(for aqueous preparations)

6.  Close 12 clean vials with the prepared closures
 Using a hypodermic needle with an external diameter of 0.8
mm inject 1 ml of water into vial and remove 1 ml of air
 Carry out this operation 4 times with new needle
 Pass the liquid in the vials through a filter with a pore size of
0.5µm
 No. of fragments NMT 10 except in the case of butyl rubber
closure where the total no. of fragments NMT 15
Tuesday, April 21, 2020
Fragmentation test
(for dry preparations)

7. 
 Close the vials with prepared closures
 For each closure, use new hypodermic needle with external
dia. of 0.8 mm & pierce the closures 10 times at a different
sites
 Immerse the vials upright in a 0.1% w/v solution of
methylene blue & reduce the external pressure by 27KPa for
10 min
 Restore the atmosphere pressure and leave the vials
immersed for 30 min
 Rinse the outside of the vials
 None of the vials contains any trace of colored solution
Tuesday, April 21, 2020
Self-seal ability

8. 
 Take 20 ml of solution A, add 0.1 ml bromothymol
blue
 Add small amount of 0.01 NaOH, after its addition
color changes from blue to yellow
 The vol. of NaOH required to change the color
should not be more than 0.3 ml and if it is done with
HCL, the volume of HCL needed should not be more
than 0.8 ml
Tuesday, April 21, 2020
pH of aqueous extract

9. 
 It must be done within 4 hr of preparing
solution A
 Solution A is filtered through 0.5µ filter and
its absorbance is measured at 220-360 nm
 Similarly, take absorbance of blank without
closures and absorbance should not be more
than 2.0
Tuesday, April 21, 2020
Light absorption test

10. 
Tuesday, April 21, 2020
Reducing substances
20 ml of
solution A
1 ml 1M
H2SO4
20 Ml of 0.002
M KMnO4
Boil for 3
minutes and
then cool
Add 1 gm of
KI
Titrated with 0.01 M sodium thio-
sulphate solution using starch as an
indicator

11. 
 Take 50 ml of solution A and evaporate to dryness at
105 ºc
 Then weigh the residue, the amount of residue
should not more than 4 mg
Tuesday, April 21, 2020
Residue on evaporation

12. 
No Name of test Description
1 Moisture content All the substances will be measure at temp specified for test
2 Folding endurance Fold the piece back and forth until rupture
3 Density For rigid cellular materials
4 Method for
determining air
permeability
Expressed in pa…s-1. important for using light weighted uncoated paper on
machine
5 Paper caliper Single sheet thickness b/w one surface and other
6 Tensile strength Maximum tensile force per unit width that a paper or board withstand before
breaking
7 Tear strength Mean force required to continue the tearing of an initial cut in a single sheet
of paper
8 Puncture resistance
test
Energy require to make initial puncture
9 stiffness Degree of resistance offered by board when it is bent
10 Cobb test Test for water absorbency
Tuesday, April 21, 2020
For secondary packaging material(Paper & Board)

13. 
No Name of test Description
11 Rub resistance Test This is resistance of printed test piece to withstand rubbing against another
similar test piece
12 Pick Test A specified amount of special oil is added to the printing system & printed on
to the test piece. The surface is examined for sign of picks
13 pH, chloride or
sulphate
Just to check life of the paper/board
14 Roughness &
smoothness
Important for printing purpose
15 Brightness Measured Reflectance at wavelength of 457 nm
16 Wet burst test It is used to determine wet bursting strength of any paper or board following
immersion in water
17 Ash in paper & board Determining of ash content in board & paper
18 Nitrogenous
substance estimation
It applies to only substances that have strong affinity for acid dyes
19 Ink absorbency Determination of ink absorption by paper & board by K& N ink
20 Wet tensile strength Determination of wet tensile strength on immersion in water
Tuesday, April 21, 2020

14. 
Tuesday, April 21, 2020